US3173949A - Recovery of glutamic acid from a fermentation broth using cation exchange resins - Google Patents
Recovery of glutamic acid from a fermentation broth using cation exchange resins Download PDFInfo
- Publication number
- US3173949A US3173949A US113078A US11307861A US3173949A US 3173949 A US3173949 A US 3173949A US 113078 A US113078 A US 113078A US 11307861 A US11307861 A US 11307861A US 3173949 A US3173949 A US 3173949A
- Authority
- US
- United States
- Prior art keywords
- glutamic acid
- fermentation broth
- exchange resin
- cation exchange
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 title claims description 44
- 235000013922 glutamic acid Nutrition 0.000 title claims description 42
- 239000004220 glutamic acid Substances 0.000 title claims description 42
- 238000000855 fermentation Methods 0.000 title claims description 16
- 230000004151 fermentation Effects 0.000 title claims description 14
- 239000003729 cation exchange resin Substances 0.000 title claims description 5
- 238000011084 recovery Methods 0.000 title description 2
- 229940023913 cation exchange resins Drugs 0.000 title 1
- 230000002378 acidificating effect Effects 0.000 claims description 24
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 150000001768 cations Chemical class 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 40
- 229960002989 glutamic acid Drugs 0.000 description 38
- 239000003456 ion exchange resin Substances 0.000 description 14
- 229920003303 ion-exchange polymer Polymers 0.000 description 14
- 238000003795 desorption Methods 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 229920001429 chelating resin Polymers 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000001455 metallic ions Chemical class 0.000 description 2
- -1 Amberlite IR-lZO Chemical compound 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P13/00—Preparation of nitrogen-containing organic compounds
- C12P13/04—Alpha- or beta- amino acids
- C12P13/14—Glutamic acid; Glutamine
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/04—Processes using organic exchangers
- B01J39/05—Processes using organic exchangers in the strongly acidic form
Definitions
- the fermentation broth of glutamic acid is admixed with a large quantity of contaminating ions, such as ammonium ion added during the culture, and unutilized ammonium ion produced by decomposition of urea or metallic ion added as a required nutriment source.
- contaminating ions such as ammonium ion added during the culture, and unutilized ammonium ion produced by decomposition of urea or metallic ion added as a required nutriment source.
- This invention relates to a method for treating a glutamic acid fermentation broth as set out above characterized by first, eliminating the contaminating ions with weak acidic ion exchange resin having a high capability of exchange and which does not adsorb glutamic acid, and second, flowing oif anions as well as non-electrolyte impurities with strong acidic ion exchange resin when treating the fermentation broth of glutamic acid or other liquids containing glutamic acid, for the purpose of removing the defects above mentioned.
- substantially all the strong acidic cations are adsorbed and eliminated by using weak acidic ion exchange resin having a large cation exchange volume in the first stage of the inventive process.
- the resultant liquid having high purity of glutamic acid, is contacted with a strong acidic ion-exchange resin whereby glutamic acid as well as a minimal quantity of cations are adsorbed and all anions are flowed off.
- a liquid having high concentration and purity of glutamic acid is recovered chromatographically by using caustic soda as a desorption agent, and the liquid is then allowed to stand for cooling to obtain crystalline glutamic acid having high purity.
- a principle of this invention is based on the facts that glutamic acid is an amphoteric electrolyte and has a property of acting either as anion or as cation according to the conditions, and that weakly acidic ion exchangers, for instance, carbonic acid exchangers, selectively adsorb cations under certain conditions and, moreover, have an extremely large capacity for exchanging or adsorbing strong cations under alkaline state, namely, as much as about 180% of strong acidic ion-exchange resin may be exchanged and adsorbed.
- weakly acidic ion exchangers for instance, carbonic acid exchangers
- cations in the fermentation broth such as ammonium ion, metallic ion, basic amino acidic ion and the like are adsorbed by introducing alkaline after-fermentation broth having a pH of about 8, obtained by removal of bacterial body or heated, through weak acidic ion exchange resin.
- alkaline after-fermentation broth having a pH of about 8 obtained by removal of bacterial body or heated, through weak acidic ion exchange resin.
- Amberlite IRC-SO Duolowing the solution to stand lite 08-101 and the like, may be used, which are previously regenerated to H-form.
- adsorption ability decreases, as weak acidic ion does not decompose neutral salt in general.
- glutamic acid in the broth is an amphoten'c electrolyte and is present as weak anion, adsorption ability is not decreased until the pH attains an isoelectric point of glutamic acid, which means that almost all cations corresponding to glutamic acid as anions can be adsorbed and removed.
- An effluent from the weak acidic resin column is then fed through strong acidic ion-exchange resin such as Amberlite IR-lZO, Duolite C-3, Diaion SK-l etc., which has been previously regenerated to H-form, to carry out adsorption of glutamic acid.
- glutamic acid acts as a Weak cation in strong acidic ion-exchange resin, it is adsorbed to a fixed layer in the resin column, apart from strong cation, a small amount of which has been mingled in the first stage.
- this adsorption layer is situated at the lowest part of the resin column, it is pushed out comparatively simply by pouring a small amount of a desorption agent from upper part of the column and is desorbed separately from other cations.
- the desorption liquid comes out as glutamic acid solution having a pH around 3.2 which is almost the isoelectric point.
- this liquid contains 3 to 5 times the glutamic acid concentration as the initial feed material and at the same time, not only are contaminating ions removed but also substances which interfere with crystallization of glutamic acid such as proteinous substances, high polymer coloring matter compounds, remained sugar after-fermentation, polymerization products of carbohydrates etc., are flowed oii when the liquid is fed through the strong acidic resin column. Therefore, the final efiluent is so pure a glutamic acid solution that it is possible to obtain crystalline glutamic acid having high purity in favorable yield by merely alfor cooling or by forcible cooling.
- Table 1 shows a balance list of. substances when strong acidic ion-exchange resin is used alone and according to this invention.
- Glu. glutamic acid.
- Sug remained sugar (as grape sugar).
- EXAMPLE 1 A liquid of glutamic acid containing 4.2 gr./dl. of pH of 8.2 was heated to 60 C. After filtration from bacterial fermentation'medium, this was press-introduced from upper part of a standing resin column filled with 200 .l. of Weak acidic ion-exchange resin or Amberlite IRG-50, which is previously regenerated to H-form. The feed of the liquid (S.V. 67) was stopped just before the pH increased rapidly to around from the initial pH of around 3. At the same time, this effluent was successively fed at S.V. 3-4 to upper part of a standing resin column filled with 400 l.
- the concentration of glutamic acid was 16.6 gr./ d1. This liquid was allowed to stand for cooling for 14 hours, then forcibly cooled to 5 C. and crystallized. This was dried after filtration by centrifugation to obtain 15.7 kg. of 98% crude crystalline glutamic acid. The mother liquor was-further concentrated to obtain 0.5 kg. of 96% crude crystalline glutamic acid. The yield ratio was 95.5%.
- Method for recovering glutamic acid from a glutamic acid-containing fermentation broth which comprises (1) charging at a space velocity of 3 to 6 glutamic acidcontaining fermentation broth having a pH of about 8 at a temperature of 30 to C. into a column containing carboxylic acid-type weakly acidic cation exchange resin of H-form while maintaining the effluent pH between 2 and 6 whereby cationic impurities in said liquid are removed,
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Biotechnology (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2566960 | 1960-05-30 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3173949A true US3173949A (en) | 1965-03-16 |
Family
ID=12172175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US113078A Expired - Lifetime US3173949A (en) | 1960-05-30 | 1961-05-29 | Recovery of glutamic acid from a fermentation broth using cation exchange resins |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US3173949A (en:Method) |
| BE (1) | BE604404A (en:Method) |
| CH (1) | CH401987A (en:Method) |
| DE (1) | DE1417603A1 (en:Method) |
| GB (1) | GB947797A (en:Method) |
| NL (2) | NL123588C (en:Method) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3331828A (en) * | 1964-09-30 | 1967-07-18 | Merck & Co Inc | Isolation of gamma-l-glutamyl dipeptides from glutamic acid fermentation broths by ion exchange |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL116848A (en) * | 1996-01-22 | 2000-06-01 | Amylum Nv | Process for producing glutamic acid |
| IL118892A (en) * | 1996-07-18 | 2000-08-13 | Amylum Nv | Process for the production of crystalline aspartic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1973574A (en) * | 1931-04-29 | 1934-09-11 | Larrowe Suzuki Company | Process for manufacturing and recovering glutamic acid |
| US2738353A (en) * | 1951-11-24 | 1956-03-13 | Int Minerals & Chem Corp | Purification and recovery of pyrrolidone carboxylic acid |
| US3015655A (en) * | 1955-07-18 | 1962-01-02 | John B Stark | Separation of nitrogenous organic compounds |
-
0
- NL NL265337D patent/NL265337A/xx unknown
- NL NL123588D patent/NL123588C/xx active
-
1961
- 1961-05-29 GB GB19375/61A patent/GB947797A/en not_active Expired
- 1961-05-29 US US113078A patent/US3173949A/en not_active Expired - Lifetime
- 1961-05-30 BE BE604404A patent/BE604404A/fr unknown
- 1961-05-30 DE DE19611417603 patent/DE1417603A1/de active Pending
- 1961-05-30 CH CH627261A patent/CH401987A/fr unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1973574A (en) * | 1931-04-29 | 1934-09-11 | Larrowe Suzuki Company | Process for manufacturing and recovering glutamic acid |
| US2738353A (en) * | 1951-11-24 | 1956-03-13 | Int Minerals & Chem Corp | Purification and recovery of pyrrolidone carboxylic acid |
| US3015655A (en) * | 1955-07-18 | 1962-01-02 | John B Stark | Separation of nitrogenous organic compounds |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3331828A (en) * | 1964-09-30 | 1967-07-18 | Merck & Co Inc | Isolation of gamma-l-glutamyl dipeptides from glutamic acid fermentation broths by ion exchange |
Also Published As
| Publication number | Publication date |
|---|---|
| BE604404A (fr) | 1961-09-18 |
| GB947797A (en) | 1964-01-29 |
| NL265337A (en:Method) | |
| CH401987A (fr) | 1965-11-15 |
| NL123588C (en:Method) | |
| DE1417603A1 (de) | 1968-10-10 |
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